CN105062478A - Biological method for preparing ferrite-bismuth ferrite composite fluorescent material - Google Patents

Biological method for preparing ferrite-bismuth ferrite composite fluorescent material Download PDF

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CN105062478A
CN105062478A CN201510486837.6A CN201510486837A CN105062478A CN 105062478 A CN105062478 A CN 105062478A CN 201510486837 A CN201510486837 A CN 201510486837A CN 105062478 A CN105062478 A CN 105062478A
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iron
ferrite
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fluorescent material
reducing bacteria
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CN105062478B (en
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边亮
李海龙
董海良
张晓艳
陈敬春
侯文平
史发年
王磊
任卫
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The present invention relates to a biological method for preparing a ferrite-bismuth ferrite composite fluorescent material. The biological method comprises three steps of: step I: in a tryptone soy broth culture medium, respectively culturing 30 g/L shewanella putrefaciens MR-1 and 30 g/L iron-reducing bacteria CN-32; step II: using a peptization reflow technique to prepare transition metal single-doped iron oxide hydroxide; and step III: under an aerobic condition at the room temperature, adding the single-doped iron oxide hydroxide and bismuth ferrite respectively into the shewanella putrefaciens MR-1 and the iron reduction bacteria CN-32, standing and layering to obtain the ferrite-bismuth ferrite nano composite fluorescent material respectively prepared from the shewanella putrefaciens MR-1 and the iron-reducing bacteria CN-32. Compared with the current conditions, the biological method for preparing the ferrite-bismuth ferrite composite fluorescent material has the advantages of a low price, a simple process, less pollution, and a high recovery rate. The ferrite-bismuth ferrite composite fluorescent material powder obtained by the method is high in purity, complete in topography, and uniform in thickness, has good fluorescent properties and can be applied to the fields of magnetic resonance imaging, targeting drug delivery, magnetic hyperthermia, and the like.

Description

A kind of biological method preparing ferrite-bismuth ferrite composite fluorescent material
Technical field
The present invention relates to a kind of biological method preparing ferrite-bismuth ferrite composite fluorescent material, belong to technical field of biological material.
Background technology
At present, magnetic and luminescent material combine the hot subject having become cell marking research, and nano-composite fluorescent material has potential application at biologic applications device, as drug delivery, and MIR and fluorescence imaging, and treatment aspect.Nano-composite fluorescent material because it have the photoelectricity special efficacy of fluorescent material and magneticsubstance concurrently can be handling, in medical field, have the application prospect of many brilliances: (1) is by utilizing nuclear magnetic resonance identification intra-operative malignant tissue and high-resolution fluorescence imaging; (2) suitably nano-composite fluorescent material particle surface can provide the stable of resistant to aggregation under at physiological ph and ionic strength, reduces the chance caught by the immunity system of human body, provides suitable avtive spot, be combined further with medicine and bio-ligand; (3) its good biocompatibility, relatively easy and organic materials, inorganic metal, and oxide material is functionalized realizes good dispersiveness, is suitable for various bioactive molecules compound functionalized further.Nano-composite fluorescent material is become the material of remarkable application prospect.
Z 250 is because preparation method is simple, and cost is lower, and magnetic is strong and be widely used in synthesis dual-functional nanometer mixture, but single ferroferric oxide nano granules easily occurs fluorescent quenching.In order to solve the fluorescent quenching problem of ferroferric oxide nano granules, transition metal and organism are to the modification of the characteristics of electrical conductivity of Z 250-bismuth ferrite heterojunction.But in nano-composite fluorescent material preparation process, traditional physics or chemical process are all difficult to avoid, because high temperature annealing produces inorganic material surface defect, lowering optomagnetic characteristic.In addition, adopt N-shaped Z 250 shell coated p-type bismuth ferrite kernel easily to cause the transformation of effective electron direction of transfer in heterojunction, the magnetic of reduction nanometer cladding and particle surface catch the speed in effective electron and hole.Therefore, in this work, adopt Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 to develop four kinds of single transient metal doped ferrite-bismuth ferrate nano composite fluorescent materials at ambient temperature respectively.The object of this work is the metal-doped impact on ferrite-bismuth ferrate nano composite fluorescent material fluorescent characteristic of research.The material of the method synthesis is compared with prior art: have hypotoxicity, low surface defect, the optomagnetic advantage such as multi-functional.
Summary of the invention
The object of the invention is, a kind of biological method preparing ferrite-bismuth ferrite composite fluorescent material is provided, the method divides three steps to carry out, the first step: in pancreas peptone soybean broth substratum, cultivates Shewanella putrefaciens MR-1 and the iron-reducing bacteria CN-32 of 30g/L respectively; Second step: adopt peptization technique of backflow to prepare the iron oxide hydroxide of transition metal list doping; 3rd step: under room temperature anaerobic condition, the iron oxide hydroxide of single doping and bismuth ferrite are added with in Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively, stratification, obtains the ferrite-bismuth ferrate nano composite fluorescent material prepared by Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively.The method is compared with existence conditions: have cheap, technique simple, pollute less, rate of recovery advantages of higher.The ferrite obtained by the method-bismuth ferrite fluorescent material powder purity is high, pattern is complete, thickness is comparatively even, has good fluorescent characteristic, can be applicable to the fields such as nuclear magnetic resonance, target administration and magnetic thermotherapy.
A kind of biological method preparing ferrite-bismuth ferrate nano composite fluorescent material of the present invention, follows these steps to carry out:
A, be Tryptones 17g at pancreas peptone soybean broth substratum, soy peptone 3g, sodium-chlor 100g, dipotassium hydrogen phosphate 2.5g, glucose 2.5g, in distilled water 1000ml, cultivate 30g/L Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively, 48 hours time, then under the freezing conditions of temperature 5 DEG C centrifugal go out Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 bacterial classification, required two kinds of microorganisms when obtaining synthesizing fluorescent material;
B, in molar ratio transition metal ion are chromium chloride, cobalt chloride, Manganous chloride tetrahydrate or nickelous chloride: iron ion is ferric chloride hexahydrate=1:2, temperature be 85 DEG C, pH value be in the aqueous nitric acid of 1.5 reflux 2 hours, stratification, centrifugal, in temperature 50 C vacuum environment, drying 20 hours, obtains single transient metal doped iron oxide hydroxide;
C, the single transient metal doped iron oxide hydroxide solution obtained in step b to be mixed with mol ratio 1:1 with bismuth ferrite solution, add the two kinds of microbial strains Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 that cultivate in step a respectively, add Mineralized Culture base corresponding to Shewanella putrefaciens MR-1 and Mineralized Culture base corresponding to iron-reducing bacteria CN-32 more respectively, regulator solution pH value is 6, and then add 1 respectively, 4-piperazine two ethyl sulfonic acid 4.5mM and anthraquinone 2,6-disulfonic acid sodium 0.1mM, alleviate cell to contact with iron oxide hydroxide powder, mix;
D, under temperature 30 DEG C of conditions, by step c two kinds of solution respectively anaerobic sealing keep in Dark Place 45 days, centrifugal, washed with de-ionized water 3 times, vacuum 70 DEG C of dryings 48 hours, obtain the ferrite-bismuth ferrate nano composite fluorescent material of the list doping of being synthesized by two kinds of bacterial classification Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32.
The Mineralized Culture base that in step c, Shewanella putrefaciens MR-1 is corresponding is: (NH 4) 2sO 49.0mM, K 2hPO 45.7mM, KH 2pO 43.3mM, NaHCO 32.0mM, MgSO 47H 2o1.01mM, CaCl 22H 2o0.485mM, Sytron 67.2 μMs, H 3bO 356.6 μMs, NaCl10.0 μM, FeSO 47H 2o5.4 μM, CoSO 45.0 μMs, Ni (NH 4) 2(SO 4) 25.0 μMs, Na 2moO 43.87 μMs, Na 2seO 41.5 μMs, MnSO 41.26 μMs, ZnSO 41.04 μMs, CuSO 40.2 μM, arginase 12 0mgL -1, L-glutamic acid 20mgL -1with Serine 20mgL -1.
The Mineralized Culture base that in step c, iron-reducing bacteria CN-32 is corresponding is: Sodium.alpha.-hydroxypropionate 18mM, NH 4cl22mM, KCl1.2mM, CaCl 20.61mM, nitrilotriacetic acid(NTA) 0.71mM, MgSO 47H 2o1.1mM, NaCl1.5mM, MnSO 4h 2o0.27mM, ZnCl 286 μMs, FeSO 47H 2o32 μM, CaCl 22H 2o61 μM, CoCl 26H 2o38 μM, Na 2moO 42H 2o9.3 μM, Na 2wO 42H 2o6.8 μM, NiCl 26H 2o9.1 μM, CuSO 45H 2o3.6 μM, AlK (SO 4) 212H 2o1.9 μM, H 3bO 315 μMs.
A kind of biological method preparing ferrite-bismuth ferrate nano composite fluorescent material of the present invention, bacterial classification Shewanella putrefaciens MR-1 described in the method, iron-reducing bacteria CN-32 is given by Midland, MI university, China University of Geosciences, Mianyang, Sichuan Dong current chart seminar of Xinan Science and Technology Univ., in May, 2014 time.
Accompanying drawing explanation
Fig. 1 is that the present invention synthesizes the scanning electron microscope (SEM) photograph of the composite fluorescent material obtained respectively through Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 bacterial classification, wherein (1) and (1 ') representative is respectively by Shewanella putrefaciens MR-1, the scanning electron microscope (SEM) photograph of the chromium list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (2) and (2 ') representative respectively by Shewanella putrefaciens MR-1, the scanning electron microscope (SEM) photograph of cobalt list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (3) and (3 ') representative respectively by Shewanella putrefaciens MR-1, the scanning electron microscope (SEM) photograph of manganese list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (4) and (4 ') representative respectively by Shewanella putrefaciens MR-1, the scanning electron microscope (SEM) photograph of nickel list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (5) and (5 ') representative respectively by Shewanella putrefaciens MR-1, the scanning electron microscope (SEM) photograph of pure Z 250-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis.
Fig. 2 is that the present invention is respectively through Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32 bacterial classification synthesizes the inversion fluorogram of composite fluorescent material under 488 nanometer lasers excite obtained, wherein (1) and (1 ') representative is respectively by Shewanella putrefaciens MR-1, the inversion fluorogram of the chromium list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (2) and (2 ') representative respectively by Shewanella putrefaciens MR-1, the inversion fluorogram of cobalt list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (3) and (3 ') representative respectively by Shewanella putrefaciens MR-1, the inversion fluorogram of manganese list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (4) and (4 ') representative respectively by Shewanella putrefaciens MR-1, the inversion fluorogram of nickel list doped ferroferric oxide-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis; (5) and (5 ') representative respectively by Shewanella putrefaciens MR-1, the inversion fluorogram of pure Z 250-bismuth ferrite of iron-reducing bacteria CN-32 bacterial classification synthesis.
Fig. 3 is that the present invention is respectively through Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32 bacterial classification synthesizes the composite fluorescent material that the obtains fluorogram under excitation wavelength is 250 nanometers and 500 nanometers, wherein (1) and (1 ') representative is respectively by Shewanella putrefaciens MR-1, the chromium that iron-reducing bacteria CN-32 bacterial classification synthesizes, cobalt, manganese or the fluorogram of nickel list doped ferroferric oxide-bismuth ferrite under excitation wavelength is 250 nanometers; (2) and (2 ') representative respectively by Shewanella putrefaciens MR-1, the chromium of iron-reducing bacteria CN-32 bacterial classification synthesis, cobalt, manganese or the fluorogram of nickel list doped ferroferric oxide-bismuth ferrite under excitation wavelength is 500 nanometers.Wherein represent pure Z 250-bismuth ferrite; represent chromium list doped ferroferric oxide-bismuth ferrite; "-" represents manganese list doped ferroferric oxide-bismuth ferrite; "--" represents cobalt list doped ferroferric oxide-bismuth ferrite; " " represents nickel list doped ferroferric oxide-bismuth ferrite.
Embodiment
Embodiment 1
A, at pancreas peptone soybean broth substratum Tryptones 17g, soy peptone 3g, sodium-chlor 100g, dipotassium hydrogen phosphate 2.5g, glucose 2.5g, in distilled water 1000ml, cultivates 48 hours by 30g/L Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively, under temperature 5 DEG C of freezing conditions centrifugal go out Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32, required two kinds of microorganisms when obtaining synthesizing fluorescent material;
B, in molar ratio for chromium: iron=1:2 takes transition metal ion CrCl 2with iron ion FeCl 3.6H 2o raw material, the pH value put at temperature 85 DEG C be 2 aqueous nitric acid there is peptization back flow reaction, solution becomes red suspension liquid from water white transparency, react stratification after 2 hours, centrifugal, temperature 50 C vacuum-drying 20 hours, obtain khaki color powdered product, i.e. the iron oxide hydroxide of transition metal chromium list doping;
C, the bacterial classification Shewanella putrefaciens MR-1 cultivated in step a and iron-reducing bacteria CN-32 to be joined respectively in iron oxide hydroxide solution and bismuth ferrite solution that mol ratio is the transition metal chromium doping that the step b of 1:1 obtains, then the Mineralized Culture base adding Shewanella putrefaciens MR-1 respectively corresponding is: (NH 4) 2sO 49.0mM, K 2hPO 45.7mM, KH 2pO 43.3mM, NaHCO 32.0mM, MgSO 47H 2o1.01mM, CaCl 22H 2o0.485mM, Sytron 67.2 μMs, H 3bO 356.6 μMs, NaCl10.0 μM, FeSO 47H 2o5.4 μM, CoSO 45.0 μMs, Ni (NH 4) 2(SO 4) 25.0 μMs, Na 2moO 43.87 μMs, Na 2seO 41.5 μMs, MnSO 41.26 μMs, ZnSO 41.04 μMs, CuSO 40.2 μM, arginase 12 0mgL -1, L-glutamic acid 20mgL -1with Serine 20mgL -1in and Mineralized Culture base corresponding to iron-reducing bacteria CN-32 be: Sodium.alpha.-hydroxypropionate 18mM, NH 4cl22mM, KCl1.2mM, CaCl 20.61mM, nitrilotriacetic acid(NTA) 0.71mM, MgSO 47H 2o1.1mM, NaCl1.5mM, MnSO 4h 2o0.27mM, ZnCl 286 μMs, FeSO 47H 2o32 μM, CaCl 22H 2o61 μM, CoCl 26H 2o38 μM, Na 2moO 42H 2o9.3 μM, Na 2wO 42H 2o6.8 μM, NiCl 26H 2o9.1 μM, CuSO 45H 2o3.6 μM, AlK (SO 4) 212H 2o1.9 μM, H 3bO 3in 15 μMs, regulator solution pH value is 6, and then adds Isosorbide-5-Nitrae-piperazine two ethyl sulfonic acid 4.5mM and anthraquinone 2,6-disulfonic acid sodium 0.1mM respectively, alleviates cell and contacts with FeO (OH) powder, mix;
D, under temperature 30 DEG C of conditions, by step c two kinds of solution respectively anaerobic sealing keep in Dark Place 45 days, centrifugal, washed with de-ionized water 3 times, vacuum 70 DEG C of dryings 48 hours, obtain the ferrite-bismuth ferrate nano composite fluorescent material of the chromium list doping of being synthesized by two kinds of bacterial classification Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32 respectively.
Embodiment 2
A, at pancreas peptone soybean broth substratum Tryptones 17g, soy peptone 3g, sodium-chlor 100g, dipotassium hydrogen phosphate 2.5g, glucose 2.5g, in distilled water 1000ml, cultivates 48 hours by 30g/L Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively, under temperature 5 DEG C of freezing conditions centrifugal go out Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32, required two kinds of microorganisms when obtaining synthesizing fluorescent material;
B, in molar ratio for cobalt: iron=1:2 takes transitional metal ion Co Cl 2(cobalt chloride) and iron ion FeCl 3.6H 2o (ferric chloride hexahydrate) raw material, the pH value put at 85 DEG C of temperature be 2 aqueous nitric acid there is peptization back flow reaction, namely there is peptization back flow reaction in reactant, solution becomes yellow suspension from water white transparency, and reaction in 2 hours terminates, stratification, centrifugal, temperature 50 C vacuum-drying 20 hours, obtains khaki color powdered product, i.e. the iron oxide hydroxide of transition metals cobalt list doping;
C, the bacterial classification Shewanella putrefaciens MR-1 cultivated in step a and iron-reducing bacteria CN-32 to be joined respectively in iron oxide hydroxide solution and bismuth ferrite solution that mol ratio is the transition metal cobalt doped that the step b of 1:1 obtains, then the Mineralized Culture base adding Shewanella putrefaciens MR-1 respectively corresponding is: (NH 4) 2sO 49.0mM, K 2hPO 45.7mM, KH 2pO 43.3mM, NaHCO 32.0mM, MgSO 47H 2o1.01mM, CaCl 22H 2o0.485mM, Sytron 67.2 μMs, H 3bO 356.6 μMs, NaCl10.0 μM, FeSO 47H 2o5.4 μM, CoSO 45.0 μMs, Ni (NH 4) 2(SO 4) 25.0 μMs, Na 2moO 43.87 μMs, Na 2seO 41.5 μMs, MnSO 41.26 μMs, ZnSO 41.04 μMs, CuSO 40.2 μM, arginase 12 0mgL -1, L-glutamic acid 20mgL -1with Serine 20mgL -1in and Mineralized Culture base corresponding to iron-reducing bacteria CN-32 be: Sodium.alpha.-hydroxypropionate 18mM, NH 4cl22mM, KCl1.2mM, CaCl 20.61mM, nitrilotriacetic acid(NTA) 0.71mM, MgSO 47H 2o1.1mM, NaCl1.5mM, MnSO 4h 2o0.27mM, ZnCl 286 μMs, FeSO 47H 2o32 μM, CaCl 22H 2o61 μM, CoCl 26H 2o38 μM, Na 2moO 42H 2o9.3 μM, Na 2wO 42H 2o6.8 μM, NiCl 26H 2o9.1 μM, CuSO 45H 2o3.6 μM, AlK (SO 4) 212H 2o1.9 μM, H 3bO 3in 15 μMs, regulator solution pH value is 6, and then adds Isosorbide-5-Nitrae-piperazine two ethyl sulfonic acid 4.5mM and anthraquinone 2,6-disulfonic acid sodium 0.1mM respectively, alleviates cell and contacts with FeO (OH) powder, mix;
D, under temperature 30 DEG C of conditions, by step c two kinds of solution respectively anaerobic sealing keep in Dark Place 45 days, solution surface color becomes khaki color suspension liquid from khaki color, khaki color powder is obtained after reaction terminates, centrifugal, washed with de-ionized water 3 times, vacuum 70 DEG C of dryings 48 hours, obtain the ferrite-bismuth ferrate nano composite fluorescent material of the cobalt list doping of being synthesized by two kinds of bacterial classification Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32 respectively.
Embodiment 3
A, at pancreas peptone soybean broth substratum Tryptones 17g, soy peptone 3g, sodium-chlor 100g, dipotassium hydrogen phosphate 2.5g, glucose 2.5g, in distilled water 1000ml, cultivates 48 hours by 30g/L Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively, under temperature 5 DEG C of freezing conditions centrifugal go out Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32, required two kinds of microorganisms when obtaining synthesizing fluorescent material;
B, in molar ratio for manganese: iron=1:2 takes transition metal ion MnCl 2(Manganous chloride tetrahydrate) and iron ion FeCl 3.6H 2o (ferric chloride hexahydrate) raw material, the pH value put at temperature 85 DEG C be 2 aqueous nitric acid reflux, namely there is peptization back flow reaction in reactant, solution becomes green suspension liquid from water white transparency, and reaction in 2 hours terminates, stratification, centrifugal, temperature 50 C vacuum-drying 20 hours, obtains khaki color powdered product, i.e. transition metal manganese list doping iron oxide hydroxide;
C, the bacterial classification Shewanella putrefaciens MR-1 cultivated in step a and iron-reducing bacteria CN-32 to be joined respectively in iron oxide hydroxide solution and bismuth ferrite solution that mol ratio is the transition metal additive Mn that the step b of 1:1 obtains, then the Mineralized Culture base adding Shewanella putrefaciens MR-1 respectively corresponding is: (NH 4) 2sO 49.0mM, K 2hPO 45.7mM, KH 2pO 43.3mM, NaHCO 32.0mM, MgSO 47H 2o1.01mM, CaCl 22H 2o0.485mM, Sytron 67.2 μMs, H 3bO 356.6 μMs, NaCl10.0 μM, FeSO 47H 2o5.4 μM, CoSO 45.0 μMs, Ni (NH 4) 2(SO 4) 25.0 μMs, Na 2moO 43.87 μMs, Na 2seO 41.5 μMs, MnSO 41.26 μMs, ZnSO 41.04 μMs, CuSO 40.2 μM, arginase 12 0mgL -1, L-glutamic acid 20mgL -1with Serine 20mgL -1in and Mineralized Culture base corresponding to iron-reducing bacteria CN-32 be: Sodium.alpha.-hydroxypropionate 18mM, NH 4cl22mM, KCl1.2mM, CaCl 20.61mM, nitrilotriacetic acid(NTA) 0.71mM, MgSO 47H 2o1.1mM, NaCl1.5mM, MnSO 4h 2o0.27mM, ZnCl 286 μMs, FeSO 47H 2o32 μM, CaCl 22H 2o61 μM, CoCl 26H 2o38 μM, Na 2moO 42H 2o9.3 μM, Na 2wO 42H 2o6.8 μM, NiCl 26H 2o9.1 μM, CuSO 45H 2o3.6 μM, AlK (SO 4) 212H 2o1.9 μM, H 3bO 3in 15 μMs, regulator solution pH value is 6, and then adds Isosorbide-5-Nitrae-piperazine two ethyl sulfonic acid 4.5mM and anthraquinone 2,6-disulfonic acid sodium 0.1mM respectively, alleviates cell and contacts with FeO (OH) powder, mix;
D, under temperature 30 DEG C of conditions, by step c two kinds of solution respectively anaerobic sealing keep in Dark Place 45 days, centrifugal, washed with de-ionized water 3 times, vacuum 70 DEG C of dryings 48 hours, obtain the ferrite-bismuth ferrate nano composite fluorescent material of the manganese list doping of being synthesized by two kinds of bacterial classification Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32 respectively.
Embodiment 4
A, be Tryptones 17g at pancreas peptone soybean broth substratum, soy peptone 3g, sodium-chlor 100g, dipotassium hydrogen phosphate 2.5g, glucose 2.5g, in distilled water 1000ml, cultivate 30g/L Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively, 48 hours time, then under the freezing conditions of temperature 5 DEG C centrifugal go out Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 bacterial classification, required two kinds of microorganisms when obtaining synthesizing fluorescent material;
B, in molar ratio 1:2 take transition metal ion NiCl 2with iron ion FeCl 3.6H 2o raw material, put into temperature 85 DEG C and pH value be 1.5 aqueous nitric acid reflux, namely there is peptization back flow reaction in reactant, solution becomes blue suspension liquid from water white transparency, and reaction in 2 hours terminates, stratification, centrifugal, temperature 50 C vacuum-drying 20 hours, obtain khaki color powdered product, i.e. the iron oxide hydroxide FeO (OH) of single transiting metal nickel doping;
C, the bacterial classification Shewanella putrefaciens MR-1 cultivated in step a and iron-reducing bacteria CN-32 to be joined respectively in iron oxide hydroxide solution and bismuth ferrite solution that mol ratio is the transiting metal nickel doping that the step b of 1:1 obtains, then the Mineralized Culture base adding Shewanella putrefaciens MR-1 respectively corresponding is: (NH 4) 2sO 49.0mM, K 2hPO 45.7mM, KH 2pO 43.3mM, NaHCO 32.0mM, MgSO 47H 2o1.01mM, CaCl 22H 2o0.485mM, Sytron 67.2 μMs, H 3bO 356.6 μMs, NaCl10.0 μM, FeSO 47H 2o5.4 μM, CoSO 45.0 μMs, Ni (NH 4) 2(SO 4) 25.0 μMs, Na 2moO 43.87 μMs, Na 2seO 41.5 μMs, MnSO 41.26 μMs, ZnSO 41.04 μMs, CuSO 40.2 μM, arginase 12 0mgL -1, L-glutamic acid 20mgL -1with Serine 20mgL -1in and Mineralized Culture base corresponding to iron-reducing bacteria CN-32 be: Sodium.alpha.-hydroxypropionate 18mM, NH 4cl22mM, KCl1.2mM, CaCl 20.61mM, nitrilotriacetic acid(NTA) 0.71mM, MgSO 47H 2o1.1mM, NaCl1.5mM, MnSO 4h 2o0.27mM, ZnCl 286 μMs, FeSO 47H 2o32 μM, CaCl 22H 2o61 μM, CoCl 26H 2o38 μM, Na 2moO 42H 2o9.3 μM, Na 2wO 42H 2o6.8 μM, NiCl 26H 2o9.1 μM, CuSO 45H 2o3.6 μM, AlK (SO 4) 212H 2o1.9 μM, H 3bO 3in 15 μMs, regulator solution pH value is 6, and then adds Isosorbide-5-Nitrae-piperazine two ethyl sulfonic acid 4.5mM and anthraquinone 2,6-disulfonic acid sodium 0.1mM respectively, alleviates cell and contacts with FeO (OH) powder, mix;
D, under temperature 30 DEG C of conditions, by step c two kinds of solution respectively anaerobic sealing keep in Dark Place 45 days, solution surface color becomes khaki color suspension liquid from light blue, khaki color powder is obtained after reaction terminates, centrifugal, washed with de-ionized water 3 times, vacuum 70 DEG C of dryings 48 hours, obtain the ferrite-bismuth ferrate nano composite fluorescent material of the nickel list doping of being synthesized by two kinds of bacterial classification Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32 respectively.
Embodiment 5
By embodiment 1-4 obtain respectively by two kinds of bacterial classification Shewanella putrefaciens MR-1, the chromium that the nickel list that iron-reducing bacteria CN-32 synthesizes adulterates, cobalt, manganese or ferrite-bismuth ferrate nano composite fluorescent material are through scanning electron microscope (SEM) photograph (Fig. 1), as can be seen from the figure product is the reactant enwrapped granule of below a large amount of 200 nanometers, illustrate that transition metal all can reduce the surface reunion of Z 250-bismuth ferrite iron-based heterojunction, improve the dispersiveness of powder.
Embodiment 6
By embodiment 1-4 obtain respectively by two kinds of bacterial classification Shewanella putrefaciens MR-1, the chromium that the nickel list that iron-reducing bacteria CN-32 synthesizes adulterates, cobalt, manganese or the inversion fluorogram (Fig. 2) of ferrite-bismuth ferrate nano composite fluorescent material under 488 nanometer lasers excite, as can be seen from the figure the soft magnetic ferrite particles that grown of the surface uniform of bismuth ferrite, the particle size of cluster is about 1 micron.

Claims (3)

1. prepare a biological method for ferrite-bismuth ferrate nano composite fluorescent material, it is characterized in that following these steps to carry out:
A, be Tryptones 17g at pancreas peptone soybean broth substratum, soy peptone 3g, sodium-chlor 100g, dipotassium hydrogen phosphate 2.5g, glucose 2.5g, in distilled water 1000ml, cultivate 30g/L Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 respectively, 48 hours time, then under the freezing conditions of temperature 5 DEG C centrifugal go out Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 bacterial classification, required two kinds of microorganisms when obtaining synthesizing fluorescent material;
B, in molar ratio transition metal ion are chromium chloride, cobalt chloride, Manganous chloride tetrahydrate or nickelous chloride: iron ion is ferric chloride hexahydrate=1:2, temperature be 85 DEG C, pH value be in the aqueous nitric acid of 1.5 reflux 2 hours, stratification, centrifugal, in temperature 50 C vacuum environment, drying 20 hours, obtains single transient metal doped iron oxide hydroxide;
C, the single transient metal doped iron oxide hydroxide solution obtained in step b to be mixed with mol ratio 1:1 with bismuth ferrite solution, add the two kinds of microbial strains Shewanella putrefaciens MR-1 and iron-reducing bacteria CN-32 that cultivate in step a respectively, add Mineralized Culture base corresponding to Shewanella putrefaciens MR-1 and Mineralized Culture base corresponding to iron-reducing bacteria CN-32 more respectively, regulator solution pH value is 6, and then add 1 respectively, 4-piperazine two ethyl sulfonic acid 4.5mM and anthraquinone 2,6-disulfonic acid sodium 0.1mM, alleviate cell to contact with iron oxide hydroxide powder, mix;
D, under temperature 30 DEG C of conditions, by step c two kinds of solution respectively anaerobic sealing keep in Dark Place 45 days, centrifugal, washed with de-ionized water 3 times, vacuum 70 DEG C of dryings 48 hours, obtain the ferrite-bismuth ferrate nano composite fluorescent material of the list doping of being synthesized by two kinds of bacterial classification Shewanella putrefaciens MR-1, iron-reducing bacteria CN-32.
2. the biological method preparing ferrite-bismuth ferrate nano composite fluorescent material according to claim 1, is characterized in that the Mineralized Culture base that in step c, Shewanella putrefaciens MR-1 is corresponding is: (NH 4) 2sO 49.0mM, K 2hPO 45.7mM, KH 2pO 43.3mM, NaHCO 32.0mM, MgSO 47H 2o1.01mM, CaCl 22H 2o0.485mM, Sytron 67.2 μMs, H 3bO 356.6 μMs, NaCl10.0 μM, FeSO 47H 2o5.4 μM, CoSO 45.0 μMs, Ni (NH 4) 2(SO 4) 25.0 μMs, Na 2moO 43.87 μMs, Na 2seO 41.5 μMs, MnSO 41.26 μMs, ZnSO 41.04 μMs, CuSO 40.2 μM, arginase 12 0mgL 1, L-glutamic acid 20mgL 1with Serine 20mgL 1.
3. the biological method preparing ferrite-bismuth ferrate nano composite fluorescent material according to claim 1, is characterized in that the Mineralized Culture base that in step c, iron-reducing bacteria CN-32 is corresponding is: Sodium.alpha.-hydroxypropionate 18mM, NH 4cl22mM, KCl1.2mM, CaCl 20.61mM, nitrilotriacetic acid(NTA) 0.71mM, MgSO 47H 2o1.1mM, NaCl1.5mM, MnSO 4h 2o0.27mM, ZnCl 286 μMs, FeSO 47H 2o32 μM, CaCl 22H 2o61 μM, CoCl 26H 2o38 μM, Na 2moO 42H 2o9.3 μM, Na 2wO 42H 2o6.8 μM, NiCl 26H 2o9.1 μM, CuSO 45H 2o3.6 μM, AlK (SO 4) 212H 2o1.9 μM, H 3bO 315 μMs.
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